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United States Patent |
5,221,794
|
Ackerman
,   et al.
|
June 22, 1993
|
Process and composition for multicomponent one hundred percent solid
fabric softeners
Abstract
The invention relates to a method of producing a mixture of a quaternary
ammonium compound, fatty acid, fatty acid ester and tertiary amine salt in
situ which is a highly functional mixture that is manufactured in a single
step reaction whereby quaternization is completed without the aid of
solvents, especially flammable solvents. The single step reaction process
eliminates separate blending of individual components. The compositions
obtained can be used as fabric softeners, in modified clays, as hair
treating compounds and as disinfectants.
Inventors:
|
Ackerman; Jeannene A. (Upper Arlington, OH);
Miller; Michael (Columbus, OH);
Whittlinger; David E. (Janesville, WI)
|
Assignee:
|
Sherex Chemical Company, Inc. (Dublin, OH)
|
Appl. No.:
|
793216 |
Filed:
|
November 7, 1991 |
Current U.S. Class: |
510/330; 510/331; 510/491; 510/500; 510/505; 510/515; 510/519; 510/520; 548/349.1; 554/1; 554/52; 554/103; 554/223; 564/204; 564/215; 564/291; 564/292; 564/294; 564/296 |
Intern'l Class: |
C07C 209/00; C07D 233/24 |
Field of Search: |
252/8.6,8.75,8.8
548/349.1
554/1,52,103,223
564/204,215,291,292,294,296
|
References Cited
U.S. Patent Documents
2474202 | Jun., 1949 | Rust | 260/404.
|
2583772 | Jan., 1952 | Gunderson | 260/404.
|
3686025 | Aug., 1972 | Morton | 252/8.
|
4237064 | Dec., 1980 | Reck | 260/459.
|
4238373 | Dec., 1980 | Hardy et al. | 252/542.
|
4851141 | Jul., 1989 | Demangeon et al. | 252/8.
|
Foreign Patent Documents |
0048163 | Mar., 1982 | EP.
| |
0345475 | Dec., 1989 | EP.
| |
Primary Examiner: Raymond; Richard L.
Attorney, Agent or Firm: Scully, Scott, Murphy and Presser
Parent Case Text
This application is a continuation of application Ser. No. 472,738, filed
on Jan. 31, 1990, now abandoned.
Claims
We claim:
1. A method of producing a mixture of quaternary ammonium compound, fatty
acid, fatty acid ester, and tertiary amine salt by reacting in a solvent
free system, a tertiary amine, quaternizing agent, and fatty acid each in
an amount so that said mixture will contain at least a quaternary ammonium
compound, fatty acid, fatty acid ester and tertiary amine salt wherein
said tertiary amine has the formula:
##STR10##
wherein R, R.sup.1 or R.sup.2 are: (1) a linear or branched chain
aliphatic saturated or unsaturated hydrocarbon group having up to about 22
carbon atoms;
(2) a hydroxy lower alkyl group;
(3) an alkyl amide alkylene group of the formula;
##STR11##
where R.sup.4 is lower alkylene and wherein R.sup.3 is (1), (2), (4) or
(5);
(4) a lower alkoxy group;
(5) a poly(oxyloweralkylene) group;
so that at least one of R, R.sup.1, R.sup.2 is one of said hydrocarbon
groups or one of said hydroxy lower alkyl groups;
or said tertiary amine is an imidazoline of the formula;
##STR12##
wherein R.sup.5 is a linear or branched chain aliphatic saturated or
unsaturated hydrocarbon group having up to about 22 carbon atoms and
R.sup.6 is a lower alkylene group,
said quaternizing agent being capable of producing a quaternary ammonium
compound having anions A.sup.- ;
said fatty acid is a linear or branched chain saturated or unsaturated
fatty acid having from about 12 to about 22 carbon atoms;
said quaternary ammonium compound having the formula:
##STR13##
and the salts of (I) and (II) wherein R.sup.- is hydrogen; said fatty
acid ester having the formula:
##STR14##
wherein R.sup.8 is a linear or branched chain, aliphatic saturated or
unsaturated hydrocarbon group having from about 11 to about 21 carbon
atoms where said tertiary amine, quaternizing agent and fatty acid are
reacted with one another in an amount so that said mixture obtained
contains about 10 wt. % to about 80 wt. % of said quaternary ammonium
compound, about 15 wt. % to about 70 wt. % of said salt, about 1 wt. % to
about 70 wt. % of said ester and about 5 wt. % to about 70 wt. % of said
fatty acid wherein the ratio of said quaternary ammonium compound to said
salt is from about 2:1 to about 1:2 on a weight basis.
2. The method of claim 1 where said amine is an imidazoline having the
formula:
##STR15##
or an amine of the formula:
##STR16##
and said quaternary ammonium compound has the formula:
##STR17##
where R.sup.9 is alkyl or alkenyls having about 8 to about 30 carbon
atoms;
R.sup.10 and R.sup.11 are independently hydrogen or alkyl having up to
about 4 carbon atoms;
R.sup.12 is alkyl having up to about 4 carbon atoms; and the salts of (III)
or (IV) where R.sup.12 on the nitrogen atom is hydrogen.
3. The method of any of claims 1 or 2 where said tertiary amine,
quaternizing agent and fatty acid are reacted with one another in an
amount so that said mixture obtained contains about 35 wt. % to about 55
wt. % of said quaternary ammonium compound, about 10 wt. % to about 30 wt.
% of said salt, about 5 wt. % to about 25 wt. % of said ester and about 15
wt. % to about 35 wt. % of said fatty acid wherein the ratio of said
quaternary ammonium compound to said salt is from about 2:1 to about 1:2
on a weight basis.
4. The method of claim 1 where said quaternary ammonium compound is (I) or
wherein R, R.sup.1 and R.sup.2 groups is a branched chain or linear,
aliphatic saturated or unsaturated hydrocarbon group having from about 12
to about 22 carbon atoms and the balance, if any, of said R, R.sup.1 and
R.sup.2 groups is a lower alkyl group.
5. The method of claim 4 where A is a lower alkyl sulfate group; and where
R, R.sup.1 and R.sup.2 is said hydrocarbon group, it is saturated.
6. As a composition of matter, a solvent free mixture of a quaternary
ammonium compound having the formula:
##STR18##
where R, R.sup.1 and R.sup.2 are (1) linear or branched chain aliphatic
saturated or unsaturated hydrocarbon group having up to about 22 carbon
atoms;
(2) a hydroxy lower alkyl group;
(3) an alkyl amido alkylene group of the formula,
##STR19##
where R.sup.4 is lower alkylene and R.sup.3 is any of R, R.sup.1 or
R.sup.2 ;
(4) a lower alkoxy group;
(5) a poly(oxyloweralkylene) group;
so that at least one of R, R.sup.1 or R.sup.2 is one of said hydrocarbon
groups or one of said hydroxy lower alkyl groups
where R.sup.5 is a linear or branched chain aliphatic saturated or
unsaturated hydrocarbon group having up to about 22 carbon atoms and
R.sup.6 is a lower alkylene group,
where A.sup.- is an anion;
a linear or branched chain saturated or unsaturated fatty acid having from
about 12 to about 22 carbon atoms;
a tertiary amine salt having formula (I) or (II) where R.sup.7 is hydrogen
and a fatty acid ester having the formula:
##STR20##
where R.sup.8 is a linear or branched chain, aliphatic saturated or
unsaturated group having from about 11 to about 21 carbon atoms.
7. The composition of claim 6 where said amine is an imidazoline having the
formula:
##STR21##
or an amine of the formula:
##STR22##
said quaternary ammonium compound has the formula
##STR23##
where R.sup.9 is alkyl or alkenyls having about 8 to about 30 carbon
atoms;
R.sup.10 and R.sup.11 are independently hydrogen or alkyl having up to
about 4 carbon atoms;
R.sup.12 is alkyl having up to about 4 carbon atoms; and the salts of (III)
or (IV) where R.sup.12 on the nitrogen atom is hydrogen.
8. The composition of any of claims 6 or 7 where said tertiary amine,
quaternizing agent and fatty acid are present in an amount of about 10 wt.
% to about 80 wt. % of said quaternary ammonium compound, about 15 wt. %
to about 70 wt. of said salt, about 1 wt. % to about 70 wt. % of said
ester and about 5 wt. % to about 70 wt. % of said fatty acid wherein the
ratio of said quaternary ammonium compound to said salt, is from about 2:1
to about 1:2 on a weight basis.
9. The composition of any of claims 6 or 7 where said tertiary amine,
quaternizing agent and fatty acid are present in an amount so that said
mixture contains about 35 wt. % to about 55 wt. % of said quaternary
ammonium compound, about 10 wt. % to about 30 wt. % of said salt, about 5
wt. % to about 25 wt. % of said ester and about 15 wt. % to about 35 wt. %
of said fatty acid wherein the ratio of said quaternary ammonium compound
to said salt is from about 2:1 to about 1:2 on a weight basis.
10. The mixture of claim 6 where said quaternary ammonium compound is (I)
and wherein at least one of said R, R.sup.1 and R.sup.2 groups is a
branched chain or linear, aliphatic saturated or unsaturated hydrocarbon
group having from about 12 to about 22 carbon atoms and the balance, if
any, of said R, R.sup.1 and R.sup.2 groups is a lower alkyl group.
11. The mixture of claim 9 where A.sup.- is a lower alkyl sulfate group
and where R, R.sup.1 and R.sup.2 is said hydrocarbon group it is
saturated.
12. A fabric softening article of manufacture comprising a fabric softening
amount of any of the mixtures of claims 6 or 7, operatively associated
with a substrate that will release said mixture to a fabric under fabric
softening conditions.
13. The article of claim 12 where said substrate is a fabric.
14. The article of claim 12 where said substrate is a porous polymeric
material.
15. A fabric cleaning composition comprising a detergent in combination
with a fabric softening amount of the mixtures of any of claims 6 or 7.
16. The composition of claim 15 where said detergent is a synthetic
detergent.
17. The composition of claim 15 where said detergent is a soap.
Description
BACKGROUND OF THE INVENTION
1. Field of the Invention
The invention relates to a method of producing a mixture of a quaternary
ammonium compound, fatty acid, fatty acid ester and tertiary amine salt in
situ which is a highly functional mixture that is manufactured in a single
step reaction whereby quaternization is completed without the aid of
solvents, especially flammable solvents The single step reaction process
eliminates separate blending of individual components.
2. Brief Description of the Prior Art
The preparation of quaternary ammonium compounds is usually conducted in
stainless steel or glass-lined equipment to which a tertiary amine is
charged and a solvent. Flammable solvents such as isopropyl alcohol are
generally used although mixtures of isopropyl alcohol and water sometimes
are employed or water alone is used. Flammable solvents are also
undesirable because they are a fire hazard and special handling procedures
are required when they are used. In many applications, these solvents have
to be stripped from the mixture when the reaction is completed because the
ultimate use of the product is in a solventless or solid form.
After the reactants are loaded into the reactor they are heated to a
temperature of about 50 to about 100.degree. C. after which a quaternizing
reagent is added. In some instances an exotherm is produced as a result of
the quaternizing reaction and the reactor and its contents have to be
cooled. The rate of addition of the quaternizing agent can also be
controlled in order to minimize or eliminate the exotherm. As noted
previously, in some instances, the solvent, if any is employed in the
quaternizing reaction is stripped from the quaternary ammonium compound
obtained since some commercial uses for the compounds are in solventless
systems. Additionally, bulk shipments of quaternary ammonium compounds
with solvents adds to transportion costs which is another reason to remove
the solvents.
The largest use for quaternary ammonium compounds is as a fabric softener
and presently accounts for more than about three quarters of the total
market for these material. Some fabric softeners are supplied as a liquid
dispersion of from about 3% to about 10% by weight of the quaternary
ammonium compound which is adapted to be added during the rinse cycle of a
commercial or home laundering operation. Another significant fabric
softening application is the utilization of quaternary ammonium compounds
in combination with a substrate such as a nonwoven fabric or a polymeric
foam such as a polyurethane foam, this substrate so treated being added to
a fabric dryer such as a clothes dryer while the fabric or clothes are
still damp. The quaternary ammonium compound is formulated usually with a
fatty acid ester which promotes the transfer of the quaternary ammonium
compound from the nonwoven or porous polymeric substrate to the fabric or
clothes.
Lastly, quaternary ammonium compounds are now being added to both solid and
liquid laundry detergent compositions so that the quaternary ammonium
compound can be incorporated as a fabric softener during the wash cycle of
fabrics or clothes. The most successfully utilized quaternary ammonium
compounds in this last respect are the dimethyl (dihydrogenated tallow)
ammonium chlorides or methyl sulfates. Other quaternary ammonium compounds
such as imidazolines and amidoamine quaternaries are also used in this
regard.
Where the quaternary ammonium compound is used on a substrate for transfer
to fabric or clothing in a fabric or clothes dryer, it has generally been
the practice to separately blend the fatty acid ester into the quaternary
ammonium compound which involves the extra manufacturing steps of
transportion, handling and blending of the fatty acid esters into the
quaternary ammonium compounds. If these steps can be eliminated a cost
savings could be realized.
Quaternary ammonium compounds are also used to manufacture organomodified
clays which may be added to drilling muds utilized in drilling oil wells,
the organomodified clay providing improved lubrication and rheological
properties of the drilling muds. These organoclays are also employed as
thixotropic agents in plastisols, organosols, paints and other protective
coatings, grease additives, foundry additives, cosmetics, resins and
printing inks. The most common quaternary ammonium compounds employed in
this regard are methyldi(hydrogenated tallow) benzylammonium chloride,
dimethyldi(hydrogenated tallow) ammonium chloride and
dimethyl(hydrogenated tallow) benzylammonium chloride.
Quaternary ammonium compounds are also employed as bactericides the most
common of which is the quaternary ammonium compound of benzylchloride and
a dimethylalkylamine, the alkyl group having from about 12 to about 16
carbon atoms as well as trimethyl alkyl ammonium chlorides where the alkyl
group is a long chain alkyl such as an octadecyl group. Additionally,
dimethyldicoconut-oil fatty ammonium chlorides are also effective
disinfectants e.g. bactericides or bacteristats, especially against
anaerobic bacteria which are sulfate reducers that are found in oil wells,
these bacteria causing severe corrosion problems and plugging of
formations which this type of quaternary ammonium compound can minimize or
eliminate. Additionally, these quaternary ammonium compounds effective
against anaerobic bacteria are also effective in removing oil from sand
stone formations in oil wells and provide a two-fold effect of functioning
not only as a bactericide but also in promoting so-called secondary
recovery of oil.
An additional use of quaternary compounds is in hair treatment because of
the antistatic effects obtained with such compounds, as well as the
increased wetting which promotes improvements in both wet and dry combing
or brushing and improves luster and feel. The most commonly used
quaternary ammonium compounds in this respect are trimethylalkylammonium
chloride, pentaethoxystearylammonium chloride,
dimethylstearylbenzylammonium chloride and dimethyldialkylammonium
chlorides.
It is therefore an object to overcome these and other difficulties
encountered in the prior art.
It is also an object of the present invention to provide a method for
manufacturing a mixture of quaternary ammonium compounds with a fatty
ester inter allia which can be used in fabric softening applications. It
is also an object of the present invention to provide such mixtures.
It is a further object of the invention to provide mixtures of quaternary
ammonium compounds with fatty acid esters, amine salts and fatty acids
that can be employed in any or all of the foregoing applications.
These and other objects have been achieved according to the present
invention which will be further understood in view of the following
description and claims.
SUMMARY OF THE INVENTION
It has been found that a highly functional mixture of a quaternary ammonium
compound, a fatty acid ester, an ammonium salt and a fatty acid can be
obtained in a single step reaction without the aid of solvents, especially
flammable solvents to thereby produce a mixture of highly functional
components. The single step reaction thereby eliminates the separate
blending of such individual components as the fatty acid ester, the
ammonium salt and the fatty acid with the quaternary ammonium compound.
The advantage of the method of the present invention is that it provides a
composition that is non-flammable and it is ready to be flaked or powdered
because of its bulk form and can be used as a fabric softener, a fabric
lubricant, a hair condition as well as an anti-static agent that can be
released from a substrate such as a nonwoven fabric or a polymeric foam.
These mixtures can also be used in combination with synthetic detergents
or as lubricant, an emulsifier, in cosmetic preparations hair conditioning
components clay modifiers, bactericidal compositions and as a floculant.
DETAILED DESCRIPTION
As noted, the invention relates to a method for producing a quaternary
ammonium mixture that is highly functional by means of a single step
reaction as well as the various compositions that can be obtained thereby
and therewith.
In its broadest aspect the invention is directed to a method of producing a
mixture of a quaternary ammonium compound, fatty acid, fatty acid ester
and tertiary amine salt by reacting a tertiary amine, quaternizing agent
and fatty acid, each in amount so that said mixture will contain at least
a quaternary ammonium compound, a fatty acid, fatty acid ester and a
tertiary amine salt. The tertiary amine employed according to the
invention has the formula:
##STR1##
where R, R.sup.1 and R.sup.2 can be any of the following in any
combination.
(1) linear or branched chain saturated or unsaturated hydrocarbon groups
having up to about 22 carbon atoms;
(2) a lower hydroxy alkyl group;
(3) an alkyl amido alkylene group of the formula:
##STR2##
where R.sup.4 is lower alkylene and R.sup.3 is any of R, R.sup.1 or
R.sup.2 ;
(4) lower alkoxy group;
(5) poly(oxyloweralkylene) group; so that at least one of R, R.sup.1 or
R.sup.2 is one of said linear or branched chain aliphatic saturated or
unsaturated hydrocarbon groups;
or said tertiary amine is an imidazoline of the formula:
##STR3##
where R.sup.5 is a linear or branched chain, aliphatic saturated or
unsaturated hydrocarbon group having up to about 22 carbon atoms and
R.sup.6 is a lower alkylene group;
said quaternizing agent being known in the art and which will produce a
quaternary ammonium compound having an anion A.sup.-. Generally these
quaternizing agents are those having the formula R.sup.7.sub.(a-b) X.sub.;
where R.sup.7 is a lower alkyl group or cyclo lower alkyl group such as
benzyl, cyclohexylmethyl, tolyl, xylyl, naphthylmethyl, and X may be a
chlorine, iodine, bromine, sulfate, methyl sulfate, carbonate, phosphate,
borate group, formate, acetate, propionate, adipate, benzoate and the like
where (a) is equal to the valence of X and (b) is from 1 to the valence of
X.
said fatty acid is a linear or branched chain aliphatic saturated or
unsaturated fatty acid having from about 12 to about 22 carbon atoms based
on coconut oil, vegetable oils, seed oils animal fats and fish oils;
Various tertiary amines that can be employed in this regard include:,
dimethylamino propyl amine, amino ethylanolamine, distearly methyl amine,
dihydrogenated tallow methyl amine, ditallow methyl amine, dimethyl
hydrogenated tallow amine, dimethyl coco amine, distearyl ethoxyethyl
amine, stearyl bis-hydroxyethyl amine, stearyl bis (polyethoxy ethanol)
amine, bis (tallowamidoethyl) 2-hydroxyethyl amine, bis (tallowamidoethyl)
2-hydroxylpropyl amine, 1-hydrogenated tallow amido ethyl -2-hydrogenated
tallow imidazoline 1-ethylene bis (2tallow, 1-methyl, imidazolinium)
dimethyl amino propyl tallow amido-amine and hydrogenated tallow
hydroxyethyl imidazoline
##STR4##
where R.sup.9, R.sup.10, R.sup.11 and R.sup.12 are subsequently defined.
The prior art also disclosed other amines that may be used such as those
described in the U.S. Patents to Marschner, U.S. Pat. No. 4,859,456;
Caswell et al., U.S. Pat. No. 4,857,213; Demangeon, U.S. Pat. No.
4,851,141 and Mermelstein et al., U.S. Pat. No. 4,844,824 all of which are
incorporated by reference (also referred to hereafter as "the prior art
cited herein.")
Imidazoline compounds that may be used are also described in Demangeon
(supra), whereas the quarternizing agents include;
dimethyl sulfate,
diethyl sulfate,
methyl chloride,
methyl bromide and
benzyl chloride as well as those cited in the prior art cited herein.
The quaternary ammonium compound thus obtained has the formula:
##STR5##
where R, R.sup.1, R.sup.2, R.sup.3, R.sup.4, R.sup.5, R.sup.6 and R.sup.7
have been defined above;
where A.sup.- is an anion based on R.sup.7 .sub.(a-b) X or equivalent
anions known in the quaternary ammonium compound art;
##STR6##
where R9 is about C8 to C30 preferably about C12 to about C18 alkyl or
akenyls
R.sup.10 and R.sup.11 are independently hydrogen or C1 to about C4 alkyl
R.sup.12 is C1 to about C4 alkyl
m is about 2 to about 3
A.sup.- is preferably an anion such as chloride, bromide, sulfate,
methosulfate, nitrite, phosphate and carbosylate (i.e., acetate, adipate,
propionate, benzoate)
##STR7##
where R.sup.9, R.sup.10, R.sup.12, m and A.sup.- have been previously
defined.
The tertiary amine salt has the formula:
##STR8##
and the fatty acid ester has the formula:
##STR9##
wherein R.sup.8 is a linear or a branched chain aliphatic saturated or
unsaturated hydrocarbon group having from about 11 to about 21 carbon
atoms.
As used throughout this specification the terms lower alkoxy, lower
alkylene and lower alkyl are intended to include compounds having up to
about 3 or about 4 carbon atoms including the various isomeric
configurations thereof e.g. t-butyl, i-butyl, i-propyl and the like and
the various mixtures thereof whether such mixtures of such groups contain
components having one, or two, or three or four carbon atoms or more and
also where such groups individually or in combination are in any of their
isomeric forms.
In another embodiment, according to the method of the invention the
tertiary amine, quaternizing agent and fatty acid are reacted with one
another each in an amount so that the mixture obtained contains from about
10 weight percent to about 80 weight percent and especially from about 35
weight percent to about 55 weight percent of said quaternary ammonium
compound, about 15 weight percent to about 70 weight percent and
especially from about 10 weight percent to about 30 weight percent of said
salt, about 1 weight percent to about 70 weight percent and especially
from about 5 weight percent to about 25 weight percent of said ester and
from about 5 weight percent to about 70 weight percent and especially from
about 15 weight percent to about 35 weight percent of said fatty acid
wherein the ratio of said quaternary ammonium compound to said salt is
from about 2:1 to about 1:2.
In one embodiment, the method of the invention is preferably practiced so
that the quaternary ammonium compound that is obtained has the structural
formula (I) wherein at least one of R, R.sup.1 and R.sup.2 is a branched
chain or linear aliphatic saturated or unsaturated hydrocarbon group
having from about 12 to about 22 carbon atoms, preferably saturated, and
especially those based on hard tallow acids (i.e. hydrogenated tallow
fatty acids) and the balance, if any of the aforesaid R, R.sup.1 and
R.sup.2 groups is a lower alkyl group and R.sup.7 is a lower alkyl group.
In another embodiment X is a sulfate group.
The invention also relates to a mixture of the various quaternary ammonium
compounds as described above in combination with the various fatty acid
esters, fatty acids, and tertiary amine salts also as described previously
and in the amounts and ratios as described previously.
The invention also relates to a fabric softening article of manufacture
comprising a fabric softening amount of any of the mixtures as described
herein operatively associated with a substrate that will release such
mixture to a fabric under fabric softening conditions encountered in a
fabric or clothes dryer and includes the use of any of the aforesaid
mixtures in a fabric softening relationship with a nonwoven or woven fiber
or a polymeric open-celled or substantially open-celled foam substrate,
such combination being prepared in a manner well known in the art. The
mixture is employed in an amount from about 0.1 to about 10 gms and
especially 1 to about 39 grms per 9 in. by 11 in. sheet.
The various polymeric foams that are employed in this respect comprise
polyurethane foams as well as any of the art known equivalent foams.
Additionally, the invention is directed to a fabric cleaning composition
comprising a detergent in combination with a fabric softening amount of
any of the mixtures described herein. These detergents can be any of the
art known anionic, cationic, nonionic or amphoteric synthetic detergents
or wetting agents that are well known in the art or a soap i.e. the
reaction product of a fatty acid with a alkaline hydroxide that is water
soluble e.g. fatty acid reaction products of sodium, potassium or ammonium
hydroxides or amines or the art known equivalents thereof.
These surfactants are further described in Kirk-Othmer, Encyclopedia of
Chemical Technoloqy, 3rd Edition Vol. 22 pp. 332-432 which is incorporated
herein by reference. Some specific detergents that are especially suitable
in this regard include:
Detergents that can be employed in this respect comprise
alkyl benzene sulfate,
sodium lauryl ether sulfate
nonyl phenyl ethoxylates and
alkyl alcohol ethoxylates as well as those noted in the prior art cited
herein.
The mixture of the invention is incorporated into the detergents (whether
solid or liquid) by blending in a manner well known in the art. The amount
of the mixture employed is any where from about 1 to about 50 and
especially from about 2 to about 30 wt. % based on the quaternary ammonium
compound and the active components of the detergent i.e. the component of
the detergent that has both organophilic and hydrophilic groups.
The following example is illustrative.
The method of the invention as well as a mixture obtained according to this
method is examplified by the preparation of a mixture employing the
following components in the indicated amounts.
______________________________________
Components M.W. Moles % by Wt.
______________________________________
Dihydrogenated Tallow-
523 1.00 56.63
Methyl-Amine
Stearic Acid 30.00
Dimethyl Sulfate
126 0.98 13.37
______________________________________
The amine was charged to a clean, dry reactor which was heated to
140.degree. F. A slight nitrogen purge was employed over the amine that
was charged to prevent it from coming into contact with any air that might
enter into the reactor during the reaction. The stearic acid was then
charged, mixed and heated to 140.degree. F. after which the dimethyl
sulfate was charged in increments sufficient to maintain the temperature
of the reaction mixture at 140-170.degree. F. The reaction is exothermic
and the end point of the reaction is indicated to some degree when an
exotherm is no longer obtained When the reaction was completed, the
resultant mixture was allowed to cool. The foregoing method produced a
reaction mixture which was analyzed by NMR analysis showing that the
mixture obtained had the following components:
______________________________________
%
______________________________________
Quaternary Ammonium compound
46
Fatty Acid 22
Tertiary Amine and Amine Salt
19
Methyl Ester 13
______________________________________
Although the invention has been described by reference to some embodiments,
it is not intended that the novel method or the mixture obtained thereby
as well as the fabric softening article of manufacture and the detergent
containing a fabric softening amount of the mixture be limited thereby but
that certain embodiments are intended being included as falling within the
broad scope and spirit of the foregoing disclosure and the following
claims.
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